高等学校化学学报

高等学校化学学报 ›› 2002, Vol. 23 ›› Issue (9): 1656.

• 研究论文 • 上一篇    下一篇

三缺位杂多阴离子α-A-PW9O349-的苯基硅衍生物的合成和晶体结构

王敬平, 李明雪, 牛景扬   

  1. 河南大学化学化工学院, 开封 475001
  • 收稿日期:2001-08-29 出版日期:2002-09-24 发布日期:2002-09-24
  • 通讯作者: 牛景扬(1964年出生),男,博士,教授,从事多酸化学及功能材料研究.E-mail:hdnjy@netease.com E-mail:hdnjy@netease.com
  • 基金资助:

    河南省杰出青年基金;河南省自然科学基金(批准号:004040300和004031800)资助

Synthesis and Crystal Structure of the Phenylsilyl Derivative of α-A-PW9O349- (TBA)3[α-A-PW9O34(PhSiO)3(PhSi)]·2H2O

WANG Jing-Ping, LI Ming-Xue, NIU Jing-Yang    

  1. School of Chemistry and Chemical Engineering, Henan University, Kaifeng 475001, China
  • Received:2001-08-29 Online:2002-09-24 Published:2002-09-24

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摘要： 合成了三缺位杂多阴离子的苯基硅衍生物(TBA)3[α-A-PW9O34(PhSiO)3(PhSi)]·2H2O(记为1,TBA为四丁基铵阳离子),并由元素分析、红外光谱、紫外光谱对化合物进行了表征,研究了化合物的热性质.结构分析结果表明,该化合物属三方晶系,空间群R3,晶胞参数a=1.41696(16)nm,b=1.42163(16)nm,c=1.41661(16)nm,α=99.801(17)°,β=99.843(17)°,γ=99.844(17)°,V=2.7111(5)nm3.Z=1,R=0.0548.该化合物的阴离子是由1个α-A-PW9单元,通过6个W—O—Si桥键与3个PhSiO单元相连,3个PhSiO又通过Si—O—Si桥键与另1个处于帽位的PhSi相连,形成饱和闭合笼形结构.

关键词: 苯基硅, 三缺位杂多阴离子, 合成, 晶体结构

Abstract: Reaction of the trivacant heteropolyanions β-A-PW9O349- with PhSiCl3 leads to the formation of the organosilyl derivative (TBA)3[α-A-PW9O34(PhSiO)3(PhSi)]·2H2O. The complex has been characterized by elemental analysis, IR and UV spectroscopy, X-ray crystallography, TG-DTA methods. Crystals of (TBA)3[α-A-PW9O34(PhSiO)3(PhSi)] are trigonal, space group R3, with unit cell parameters: a=1.41696(16) nm, b=1.42163(16) nm, c=1.41661(16) nm, α=99.801(17)°, β=99.843(17)°, γ=99.844(17)°, V=2.7111(5) nm3. Z=1, R=0.0548. The anion consists of one α-A-PW9O349- framework which are grafted by three PhSiOgroups through six Si—O—W bridges, each of which is attached to the fourth PhSiO through three Si—O—Si bridges and become saturated closed cage structure.

Key words: Phenylsilicion, Trivacant heteropolyanion, Synthesis, Crystal structure

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